首页|期刊导航|食品工业科技|基于复合QuEChERS净化和UPLC-MS/MS的禽蛋多类禁限用兽药残留筛查与定量分析

基于复合QuEChERS净化和UPLC-MS/MS的禽蛋多类禁限用兽药残留筛查与定量分析OA

Screening and Quantitative Analysis of Multiple Classes of Prohibited/Restricted Veterinary Drug Residues in Poultry Eggs Based on Composite QuEChERS Purification and UPLC-MS/MS

中文摘要英文摘要

针对禽蛋产品中兽药残留监管所面临的多类别、高通量检测技术需求,以及现有方法在检测种类、灵敏度或基质适用性上的不足,本研究旨在建立一种可同时检测鸡蛋、鸭蛋、鹅蛋和鸽蛋中 9类 53种禁限用兽药的高通量分析方法.通过系统优化提取溶剂与QuEChERS净化材料,最终确定以0.2 mol/L Na2EDTA-Mcllvaine缓冲溶液-乙腈进行提取,采用 C18、NH2 和 PSA复合净化材料进行 QuEChERS净化,结合超高效液相色谱-串联质谱技术进行分析.结果表明,53种兽药线性关系良好(R2≥0.9903),方法检出限和定量限分别为1~4 μg/kg和2~10 μg/kg,均满足或优于 GB 31650.1-2022《食品安全国家标准 食品中 41种兽药最大残留限量》的限量要求.在 3个加标水平下,平均回收率为 61.2%~113.6%,相对标准偏差为 0.1%~18.9%.将本方法应用于 53批实际禽蛋样品的检测,在 8批样品中检出目标物,与国家标准方法的测定结果具有良好的一致性.本研究建立的方法成功解决了因药物理化性质差异大和禽蛋基质复杂导致的同步检测难题,具有前处理简便、分析速度快(10 min)、灵敏度高和准确可靠的优点,适用于多种禽蛋基质中多类别兽药残留的高通量筛查与精准监管.

To address the growing need for multi-class,high-throughput monitoring of veterinary drug residues in poultry egg products and the deficiencies of existing methods in detection scope,sensitivity and matrix applicability,a comprehen-sive method for the simultaneous determination of 53 banned and restricted veterinary drugs from 9 classes in chicken,duck,goose,and pigeon eggs was developed.The sample preparation procedure was systematically optimized,including the extraction solvent and QuEChERS purification sorbents.The optimized method involved extraction with 0.2 mol/L Na2EDTA-Mcllvaine buffer solution and acetonitrile,followed by cleanup using a composite of C18,NH2,and PSA sor-bents.The target analytes were then determined by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The results showed that all 53 veterinary drugs exhibited good linearity(R2≥0.9903).The limits of detec-tion(LOD)and the limits of quantification(LOQ)ranged from 1 μg/kg to 4 μg/kg and 2 μg/kg to 10 μg/kg,respectively,which all met or exceeded the maximum residue limits specified in the GB 31650.1-2022 National food safety standard-Maximum residue limits for 41 veterinary drugs in foods.Average recoveries at three spiked levels ranged from 61.2%to 113.6%,with relative standard deviations(RSDs)between 0.1%and 18.9%.The developed method was successfully applied to screen 53 batches of actual poultry egg samples,and eight batches were found to contain target compounds,and the results were consistent with those obtained by the national standard methods.The proposed method successfully solves the problem of simultaneous detection caused by large differences in the physical and chemical properties of drugs and complex poultry egg matrices,and has the advantages of simple sample pretreatment,fast analysis speed(10 min),high sensitivity,accuracy and reliability.It is suitable for high-throughput screening and precise supervision of multi-class vet-erinary drug residues in various poultry egg matrices.

张静;马丽娜;刘茵茵;周倩;万玉;高玉时;唐修君

江苏省家禽科学研究所,江苏 扬州 225125江苏省家禽科学研究所,江苏 扬州 225125江苏省家禽科学研究所,江苏 扬州 225125江苏省家禽科学研究所,江苏 扬州 225125江苏省家禽科学研究所,江苏 扬州 225125江苏省家禽科学研究所,江苏 扬州 225125江苏省家禽科学研究所,江苏 扬州 225125

轻工纺织

复合QuEChERS净化超高效液相色谱-串联质谱禁限用兽药禽蛋

composite QuEChERS purificationultra-performance liquid chromatography-tandem mass spectrometrybanned and restricted veterinary drugspoultry eggs

《食品工业科技》 2026 (19)

43-52,10

农产品质量安全风险评估(20254071).

10.13386/j.issn1002-0306.2025120027

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